CN105753497A - Preparation method of super-hydrophilic super-oleophilic three-dimensional graphene foam material - Google Patents
Preparation method of super-hydrophilic super-oleophilic three-dimensional graphene foam material Download PDFInfo
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Abstract
The invention discloses a preparation method of a super-hydrophilic super-oleophilic three-dimensional graphene foam material.The preparation method includes following steps: 1), adopting a classic Hummers and Offema method to prepare oxidized graphene from natural graphene powder to obtain a dispersive oxidized graphene water solution; 2), placing the oxidized graphene water solution obtained in the step 1) in a reaction kettle, dropwise adding a phytic acid solution in corresponding dosage, embedding the reaction kettle in a stainless steel jacket, disposing the stainless steel jacket in an oven for heating, maintaining 180 DEG C, reacting for 12 h, and naturally cooling to room temperature; freeze-drying a product for 24 h to obtain a cylindrical phytic acid doped super-hydrophilic super-oleophilic three-dimensional graphene foam material.The three-dimensional graphene foam material obtained by the preparation method has special property of zero contact angle to water and oil solutions, is efficient in adsorption and gathering of water, various oil liquids and various organic liquids and can be recycled through simple thermal treatment.
Description
Technical field
The present invention relates to the three-dimensional graphene foam material preparation method of a kind of super hydrophilic super oleophylic simultaneously.
Background technology
Graphene is the planar stratified material with honeycomb crystal lattice structure.Owing to having the performances such as fabulous electricity, optics, machinery, Graphene is extensively concerned.Three-dimensional grapheme typically refers to the two-dimensional graphene assembly with three dimensional structure, is the new function material of recent Graphene chemical field.Two-dimensional graphene sheet is integrated into the assembly with three dimensional structure can the electricity of Effective Regulation Graphene, optics, machinery, catalysis and surface wettability, therefore three-dimensional grapheme material not only has the physicochemical property that Graphene is intrinsic, and its three-dimensional porous micro/nano structure also has concurrently such as good characteristics such as pliability, porous, high activity specific surface area, excellent mass-transfer performances.Researcheres utilize hydro-thermal method, vapour deposition process, template synthesis method etc. to be successfully prepared the multiple three-dimensional grapheme material with micro/nano structure, wherein hydrothermal synthesis method easily operates with it, pollutes little feature and is widely used in the synthesis of three-dimensional grapheme.Additionally, Graphene can obtain composite with the effective compound of other functional materials in three-dimensional micro/nano structure forming process.Research shows, three-dimensional grapheme and composite thereof possess the character that Graphene is intrinsic, has the performance more superior compared with two-dimensional graphene material and broader practice prospect in energy storage, catalytic reaction, environmental conservation and control surface wettability etc..Currently, report about the surface wettability of three-dimensional grapheme mostly is single hydrophobic or super-hydrophobic three-dimensional grapheme infiltrated, this be due to oxidation of precursor Graphene (GrapheneOxide) in course of reaction due to sheet interlayer Π Π pile up and hydrophobic interaction, there occurs irreversible reunion and stacking, and also do not have been reported that about the three-dimensional graphene foam material with both double; two imbibition characteristics of hydrophilic oleophylic.
Summary of the invention
The purpose of the present invention, it is to provide for the three-dimensional graphene foam material preparation method of a kind of super hydrophilic super oleophylic simultaneously, the super parents' three-dimensional graphene foam material of gained of the present invention is loose porous, water, oily substance there is higher adsorption capacity, can be applicable to, to the absorption of pollutant in water surface, inside or other environment and enrichment, there is good using value and market prospect.The present invention is simple, safety and environmental protection, can be used for producing in enormous quantities.
The present invention is achieved in that the three-dimensional graphene foam material preparation method of described a kind of super hydrophilic super oleophylic simultaneously, comprises the following steps:
1) preparation of graphene oxide:
Adopt classical HummersandOffema method to prepare graphene oxide from natural graphite powder, obtain scattered graphene oxide water solution；
2) preparation of the three-dimensional graphene foam material of super hydrophilic super oleophylic simultaneously:
The graphene oxide water solution obtained in step 1) is put in reactor, and drips the plant acid solution of corresponding dosage, reactor is embedded in stainless steel outer sleeve, be placed in baking oven and heat, keep 180oC, after reaction 12h, naturally cool to room temperature；By product lyophilization 24h, obtain the three-dimensional graphene foam material of the super hydrophilic super oleophylic simultaneously of cylindric phytic acid doping.
The design source of the present invention is: will build the three-dimensional grapheme of a kind of parents, require its three-dimensional net structure exists hydrophilic and lipophilic group, the formation of super parents is then the capillary structure simultaneously building network-like crosslinking on the basis of the binary synergetic structure of hydrophilic/oil, in order to forms capillary effect and then promotes super immersional wetting.Phytic acid (phyticacid, phytic acid), is widely present in oil plant and seed corn, is the major storage form as phosphorus in various plants tissue, and its structure is the inositol derivative that 6 hydroxyls of inositol are all generated by Phosphation.The feature of phytic acid molecular structure and physicochemical property and Nantural non-toxic owing to having uniqueness, therefore, the present invention selects natural phytate molecule as gel, adulterant and coating material, with graphite oxide alkene reaction, obtained the three-dimensional graphene foam material of a kind of novel super hydrophilic super oleophylic simultaneously by the straightforward procedure of Hydrothermal Synthesis.
The invention has the beneficial effects as follows, utilize phytic acid and graphene oxide, prepare the parental type three-dimensional graphene foam material of a kind of super hydrophilic super oleophylic simultaneously, overcome the single infiltrating deficiency of existing three-dimensional grapheme macroscopic material.Gained three-dimensional graphene foam material of the present invention has the special nature that can realize that water class, oil solutions all have zero contact angle, efficient absorption and enrichment to water, multiple oil type liquid and multiple organic liquid, owing to its mechanical performance is high, by simple heat treatment, super parental type three-dimensional graphene foam material can be recycled.
Accompanying drawing explanation
Fig. 1 is the photo figure in kind of super parents' three-dimensional graphene foam material of the present invention.
Fig. 2 is the composition principle figure of super parents' three-dimensional graphene foam material of the present invention.
Fig. 3 is the scanning electron microscope (SEM) photograph of super parents' three-dimensional graphene foam material of the present invention.
Fig. 4 is the transmission electron microscope picture of super parents' three-dimensional graphene foam material of the present invention.
Fig. 5 is the X-ray diffractogram of super parents' three-dimensional graphene foam material of the present invention.
Fig. 6 is that super parents' three-dimensional graphene foam material of the present invention is to water contact angle test figure.
Fig. 7 is that super parents' three-dimensional graphene foam material of the present invention is to oil contact angle test figure.
Fig. 8 is the process photo figure that water, oil are adsorbed by super parents' three-dimensional graphene foam material of the present invention simultaneously.
Fig. 9 is that super parents' three-dimensional graphene foam material of the present invention first adsorbs water then the process photo figure of adsorbed oil.
Figure 10 is the super parents' grapheme foam material of the different quality ratio adsorption capacity comparison diagram to water.
Figure 11 is the super parents' grapheme foam material of the different quality ratio adsorption capacity comparison diagram to oil.
Figure 12 is the super parents' three-dimensional graphene foam material of the present invention mass adsorption Capacity Plan to not same solution.
Figure 13 is the super parents' three-dimensional graphene foam material of the present invention volumetric adsorption capacity figure to not same solution.
Figure 14 is the super parents' three-dimensional graphene foam material of the present invention circulation absorption test figure to water.(wherein adsorb saturated after three-dimensional graphene foam material recycle after dried).
Figure 15 is the super parents' three-dimensional graphene foam material of the present invention circulation absorption test figure to ethanol.(wherein adsorb saturated after three-dimensional graphene foam material recycle after burn processing).
Figure 16 is the super parents' three-dimensional graphene foam material of the present invention circulation absorption test figure to chloroform.(wherein adsorb saturated after three-dimensional graphene foam material through distillation process after recycling).
Detailed description of the invention
The three-dimensional graphene foam material preparation method of a kind of super hydrophilic super oleophylic simultaneously of the present invention, comprises the following steps:
1) preparation of graphene oxide:
Adopt classical HummersandOffema method to prepare graphene oxide from natural graphite powder, obtain scattered graphene oxide water solution；
2) preparation of the three-dimensional graphene foam material of super hydrophilic super oleophylic simultaneously:
The graphene oxide water solution obtained in step 1) is put in reactor, and drips the plant acid solution of corresponding dosage, reactor is embedded in stainless steel outer sleeve, be placed in baking oven and heat, keep 180oC, after reaction 12h, naturally cool to room temperature；By product lyophilization 24h, obtain the three-dimensional graphene foam material of the super hydrophilic super oleophylic simultaneously of cylindric phytic acid doping.
The present invention is further illustrated in conjunction with accompanying drawing 1-16 for following example.
The first step, prepares graphene oxide.
Classical HummersandOffema method is adopted to prepare graphene oxide from natural graphite powder.It is summarized as follows: by 2g graphite, 1gNaNO3H dense with 46mL2SO4Join in three-necked bottle, ice bath stirs 4h, is slow added into 6gKMnO afterwards4, after adding, remove rapidly ice bath, now solution is suspended aqueous, continues stirring 2h, is then slowly added into the H of 92mL2O, heats 15min in 98oC water-bath, is sequentially added into 200mL hot water and 20mLH afterwards2O2, after mix homogeneously, this mixed liquor is centrifuged under 7000rpm, and washes respectively 6 times with HCl and water, finally, concentrated solution is dried under 37oC 48h, obtains the graphite oxide ene product of lamellar.
Second step, the preparation of the three-dimensional graphene foam material of super hydrophilic super oleophylic simultaneously.
Take 150.0mg graphene oxide solid ultrasonic disperse in 30.0mL aqueous solution, obtain uniform 5.0mg/mL graphene oxide suspension.Pipette 6.0mL graphene oxide suspension respectively in 5 hydrothermal reaction kettles, move into 0 successively, 0.2,0.5,1.0,2.0mL phytic acid aqueous solution (during reaction in system phytic acid content be 0,0.22,0.55,1.1,2.2mmol), dilute with ultra-pure water again until overall solution volume is 15.0mL in each hydrothermal reaction kettle, ultrasonic 30min, now the concentration of graphene oxide is 2mg/mL, and the pH of mixed solution is about 3.0.Hydrothermal reaction kettle is screwed, puts in heated oven, start to warm up to 180oC from 25.0oC, keep 180oC, naturally cool to room temperature after 12h, columned super parents' three-dimensional grapheme hydrogel that pattern is complete can be obtained, its lyophilization 24h can be obtained super parents' three-dimensional graphene foam.
What Fig. 1 gave gained is followed successively by, containing phytic acid content, super parents' three-dimensional grapheme hydrogel that the graphene oxide mixed solution hydro-thermal reaction of (from left to right) 0,0.22,0.55,1.1 and 2.2mmol and 2mg/mL obtains, be can be seen that by Fig. 1, along with the amount adding phytic acid increases, the volume of synthetic product is gradually increased, and porousness is also gradually increased.This is owing to the increase of phytic acid makes the phosphorus hydroxyl of functionalization increase, and increases and the probability of graphite oxide alkene reaction so that graphene sheet layer increases further, in order to holding more hydrone, therefore volume increases to some extent.
3rd step, material characterization.
Phytic acid and graphene oxide all contain the oxygen-containing functional groups such as hydroxyl, reacted by hydrothermal reduction, polyhydric phytate molecule is doped in reduced form stannic oxide/graphene nano sheet, by the chemical action such as hydrogen bond formed can hydrophilic again can the three-dimensional composite material of oleophylic, its composition principle is as shown in Figure 2.
Products therefrom in second step is scanned Electronic Speculum characterize, for 2mg/mL graphene oxide and 0.5mL reaction of phytic acid product, the visible Fig. 3-5 of its internal structure.Fig. 3 is the scanning electron microscope (SEM) photograph (S4800, accelerating potential 15kv) of super parents' three-dimensional graphene foam material internal structure of gained of the present invention, by Fig. 3 it can be seen that this super parents' grapheme foam material internal present three-dimensional network crosslinking, loose porous structure；Fig. 4 is the transmission electron microscope picture (JEM-1400, accelerating potential 120kV) of super parents' three-dimensional grapheme material internal structure of gained of the present invention, it is seen that this super parents' three-dimensional grapheme has the network structure of stacking accordion；Fig. 5 is the X-ray diffractogram of the super parents' three-dimensional graphene foam material of gained of the present invention, in order to further appreciate that crystalline structure and the shape information of this super parents' three-dimensional grapheme material, this super parents' three-dimensional graphene foam material and the grapheme foam (namely 0mL phytic acid and graphite oxide alkene reaction are through Hydrothermal Synthesis products therefrom) being not added with phytic acid are carried out X-ray diffraction relative analysis.Can be drawn a conclusion: the super parents' three-dimensional graphene foam known to the present invention does not have graphene oxide 2 θ=11.34o peak, illustrate that graphene oxide is reduced in water-heat process, super parents' material obtained by the present invention also has the characteristic diffraction peak (2 θ=25o) of three-dimensional grapheme simultaneously, and slightly offset from the peak of standard three-dimensional Graphene, show owing to being phytic acid doping in water-heat process so that Graphene interplanar distance distance increases to some extent.
For verifying its parent/hydrophobicity, prepared product is carried out water/oil contact angle test (Ram é Hart200-F1goniometer), for 2mg/mL graphene oxide and 0.5mL plant acid solution gained three-dimensional graphene foam, it is to water, oil contact angle test result as shown in Figure 6,7, wherein Fig. 6 is that contact angle becomes 0 in 1.06s to water (2 μ L) contact angleo, illustrate that it has super hydrophilic character；Fig. 7 is that contact angle becomes 0 in 1.22s to oil (2 μ L) contact angleo, illustrate that it has super-oleophilic matter.In sum, gained three-dimensional graphene foam material of the present invention has double; two imbibition characteristics of super hydrophilic super oleophylic.Water, oil contact angle are become 0oTime used is different, it may be possible to owing to the viscosity institute difference of water, oil causes.
For verifying the performance of the super hydrophilic and super oleophylic of gained three-dimensional graphene foam material of the present invention further, for 2mg/mL graphene oxide and 0.5mL plant acid solution gained three-dimensional graphene foam material, verify its adsorption effect to water and oil.Fig. 8 is that this three-dimensional graphene foam material adsorbs water and the process photo figure of oil simultaneously；Fig. 9 is the process photo figure (wherein, oil is dark to observe) that this three-dimensional graphene foam material first adsorbs water adsorbed oil again.
4th step, the super parents' three-dimensional graphene foam material of the different quality ratio synthesis volumetric adsorption measure of merit to water and oil.
In the graphite alkene foam of synthesis, use 2mg/mLGO(GrapheneOxide graphene oxide) respectively with 0.22,0.55,1.1, its adsorption capacity to water oil of three-dimensional graphene foam testing of materials of 2.2mmol reaction of phytic acid, and compare its adsorption effect.This experiment at room temperature carries out, and takes column type three-dimensional graphene foam material, weighs its mass M with precision balance (METTLERTOLEDOXS205)1, then this three-dimensional graphene foam material is immersed in water/oil, three-dimensional graphene foam material can adsorbed target solution voluntarily, be drawn off after about 5 minutes, with filter paper, the solution of its excess surface removed, and then put into precision balance weighs its mass M2, then its mass adsorption capacity can be expressed as: (M2-M1)/M1, because every kind of liquid has different density, so volumetric adsorption capacity can reflect this three-dimensional graphene foam material adsorption capacity to not same solution more accurately.Its volume capacity can be expressed as: (V2-V1)/V1, wherein the volume of cylindric three-dimensional graphene foam material can pass through V=L Π D2/ 4(L is the cylinder length of side, and D is cylinder disc diameter), and the volume of variety classes liquid can be obtained by V=M/ ρ, wherein density p can be checked in by sample parameters.Through test and calculate phytic acid/volumetric adsorption effectiveness comparison such as Figure 10 of graphene oxide parents' three-dimensional graphene foam material of gained different quality ratio, shown in 11, being appreciated that the three-dimensional graphene foam material obtained by 2mg/mLGO and 0.22mmol phytic acid has best adsorption capacity, therefore we test it to the adsorption capacity of the liquid such as water of number of different types, oils not of the same race and organic solvent not of the same race and its circulation absorption effect to several representative solutions for the three-dimensional graphene foam material obtained by 2mg/mLGO and 0.22mmol phytic acid.
5th step, to water, multiple oils, gas chromatography capacity indicator.
In the multiple three-dimensional graphene foam material of the present embodiment second step synthesis, for the three-dimensional graphene foam material of 2mg/mLGO and 0.5mLPA synthesis, test it and different types of liquid is included water, commercialization oil (gasoline and pump oil), vegetable and animals oils (olive oil and Oleum Arachidis hypogaeae semen), the fragrance same clan (benzene and toluene), the quality of hydro carbons (octane, decane and dodecane) and volumetric adsorption capacity.This experiment at room temperature carries out, and takes column type three-dimensional graphene foam material, weighs its mass M with precision balance (METTLERTOLEDOXS205)1Then this three-dimensional graphene foam material is immersed in target liq, three-dimensional graphene foam material can adsorbed target solution voluntarily, be drawn off after about 5 minutes, with filter paper, the solution of its excess surface is removed, and then put into precision balance weighs its mass M2, then its mass adsorption capacity can be expressed as: (M2-M1)/M1, because every kind of liquid has different density, so volumetric adsorption capacity can reflect this three-dimensional graphene foam material adsorption capacity to not same solution more accurately.Its volume capacity can be expressed as: (V2-V1)/V1, wherein the volume of cylindric three-dimensional graphene foam material can pass through V=L Π D2/ 4(L is the cylinder length of side, and D is cylinder disc diameter), and the volume of variety classes liquid can be obtained by V=M/ ρ, wherein density p can be checked in by sample parameters.Through test with calculate gained parents' three-dimensional graphene foam material to the quality of variety classes liquid and volumetric adsorption effect as shown in Figure 12,13, it is seen that water/oil/organic pollution is all had very high mass adsorption capacity and volumetric adsorption capacity by super parents' three-dimensional graphene foam material prepared by the present invention.
5th step, tests the circulation absorption of water, ethanol, chloroform.
In the multiple three-dimensional graphene foam material of the present embodiment second step synthesis, for the three-dimensional graphene foam material of 2mg/mLGO and 0.5mL phytic acid synthesis, test its circulation absorption performance that different types of liquid is included water, ethanol and chloroform.Concrete operations are as follows: take parents' three-dimensional graphene foam material, weigh and record its quality, this three-dimensional graphene foam material is immersed in target liquid (respectively water, ethanol and chloroform), three-dimensional graphene foam material can adsorbed target solution voluntarily, it is drawn off after about 5 minutes, with filter paper, the solution of its excess surface is removed, measure quality after it adsorbs with precision balance, again weigh three-dimensional graphene foam quality of materials record after drying.Dried three-dimensional graphene foam material is replaced in target liquid again, re-covers aforesaid operations, record the quality before and after its absorption, and draw circulation absorption design sketch.Wherein dry method is respectively as follows: (1) and is adsorbed with the three-dimensional graphene foam material use baking oven of water 60oDry 24h when C；(2) it is adsorbed with after the three-dimensional graphene foam material alcohol burner of ethanol lighted, utilizes combustion method to dry；(3) method of the three-dimensional graphene foam material use distillation being adsorbed with chloroform is dried.As shown in Figure 14,15,16, multiple different liquids pollutant are not only had higher adsorption capacity by super parents' three-dimensional graphene foam material prepared by the present invention, and the purpose recycled can be reached, even if after repeatedly recycling, still there is good adsorption effect.
Compared with existing macroscopic three dimensional grapheme material, super parents' three-dimensional graphene foam material of gained of the present invention and preparation method thereof has following characteristics:
(1) the invention discloses and a kind of prepare the not only hydrophilic but also method of the parental type three-dimensional graphene foam material of oleophylic, with simple hydrothermal synthesis method, one-step synthesis surpasses parents' three-dimensional graphene foam material.Preparation method economy, simple, can be used for large-scale production.
(2) present invention choose avirulence, environmental protection phytic acid as reducing agent, when Hydrothermal Synthesis, self assembly autohemagglutination is combined into porous network shape structure.Owing to this structure contains a large amount of hydrophilic phosphorus hydroxyl groups from phytic acid, and contain hydrophobic conjugation benzene ring structure by the reduced form graphene oxide after hydrothermal reduction so that this three-dimensional grapheme have can hydrophilic again can the microstructure of oleophylic.Water and oil based solvent contact angle are zero by obtained three-dimensional graphene foam material, namely have the feature of super hydrophilic and super oleophylic simultaneously.Additionally, this super parents' three-dimensional graphene foam material also has the advantages such as high temperature resistant, mechanical strength is high, reusable.
(3) water/oil based solvent is all had significantly high adsorption capacity by super parents' three-dimensional graphene foam material prepared by the present invention, it is possible to be applied to enrichment to environmental pollutants and absorption, especially the absorption of water body, marine pollutant.Conventional three-dimensional grapheme can only adsorb oily substance or hydrophobic organic liquid, and the shortcoming that super parents' three-dimensional graphene foam material of gained of the present invention overcomes the three-dimensional grapheme of single infiltration in the past, it is possible not only to adsorb the oil of hydrophobic Organic substance or leakage, it is also possible to be applied to water surface and the absorption of internal contamination thing.
(4) adsorption capacity of water/oils can be regulated and controled by super parents' three-dimensional graphene foam material prepared by the present invention by the ratio of precursors graphene oxide and phytic acid.And adsorb saturated after super parents' three-dimensional graphene foam material can be processed by simple heat treatment or distillation and remove its solvent adsorbed so that this super parents' three-dimensional graphene foam material can repetitive cycling use.
Claims (1)
1. a three-dimensional graphene foam material preparation method for super hydrophilic super oleophylic simultaneously, comprises the following steps:
(1) preparation of graphene oxide:
Adopt classical HummersandOffema method to prepare graphene oxide from natural graphite powder, obtain scattered graphene oxide water solution；
(2) preparation of the three-dimensional graphene foam material of super hydrophilic super oleophylic simultaneously:
The graphene oxide water solution obtained in step (1) is put in reactor, and drips the plant acid solution of corresponding dosage, reactor is embedded in stainless steel outer sleeve, be placed in baking oven and heat, keep 180oC, after reaction 12h, naturally cool to room temperature；By product lyophilization 24h, obtain the three-dimensional graphene foam material of the super hydrophilic super oleophylic simultaneously of cylindric phytic acid doping.
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| CN107674236A (en) * | 2017-11-07 | 2018-02-09 | 中国科学院金属研究所 | A kind of super parents' polyurethane foamed material and preparation method thereof |
| CN108314015A (en) * | 2018-03-16 | 2018-07-24 | 江南大学 | A kind of preparation method of functionalization graphene aerogel microball |
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| CN108467033A (en) * | 2018-03-13 | 2018-08-31 | 镇江致达新材料科技有限公司 | A kind of preparation method of bionic laminar nano composite film |
| CN108314015A (en) * | 2018-03-16 | 2018-07-24 | 江南大学 | A kind of preparation method of functionalization graphene aerogel microball |
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| CN113773067A (en) * | 2021-11-11 | 2021-12-10 | 长沙中瓷新材料科技有限公司 | Sagger based on cordierite and production process thereof |
| CN113773067B (en) * | 2021-11-11 | 2022-01-18 | 长沙中瓷新材料科技有限公司 | Sagger based on cordierite and production process thereof |
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